CN102883999B - Silica containing particle - Google Patents

Silica containing particle Download PDF

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Publication number
CN102883999B
CN102883999B CN201180023167.4A CN201180023167A CN102883999B CN 102883999 B CN102883999 B CN 102883999B CN 201180023167 A CN201180023167 A CN 201180023167A CN 102883999 B CN102883999 B CN 102883999B
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organosilane
composition
mol ratio
compound
alternatively
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CN102883999A (en
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布鲁斯·A·凯泽
尼古拉斯·S·埃冈
理查德·米姆纳
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ChampionX LLC
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Ondeo Nalco Co
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
    • A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
    • A23L2/80—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/08—Silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/12—Silica and alumina
    • B01J35/615—
    • B01J35/635—
    • B01J35/638—
    • B01J35/647—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume

Abstract

The invention discloses a kind of silica containing composition.Described silicon dioxide compositions comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide.

Description

Silica containing particle
Technical field
The present invention relates to a kind of silica containing composition.
Background technology
Material containing silicon-dioxide has a wide range of applications.More specifically, the multiple manufacture method of productive consumption product or Industrial products, uses the material containing silicon-dioxide for different objects.Such as, the product containing silicon-dioxide can be used as filler, support of the catalyst, beer/grape wine/fruit juice clarifier in coating (as paint) and polymer composites.New strengthen the property with having of improving and the silica containing product of ease for use needed for every profession and trade.
Summary of the invention
A. composition
The invention provides a kind of composition, described composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein, M exists alternatively and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide.
In one embodiment, the mol ratio of x/z be following at least one: 0.56,3.5 and 5.5.
B. the product obtained by method
Present invention also offers a kind of by filtering the obtained product of water-based material from composition, described composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide, and in water-based slurry, wherein comprise the described composition of 3 % by weight to 15 % by weight.
Present invention also offers a kind of by the obtained product of the temperature drying composition of 100 ° of C to 350 ° of C, wherein said composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide.
For these two kinds of products, in one embodiment, the mol ratio of x/z be following at least one: 0.56,3.5 and 5.5.
C. manufacture method
The invention provides a kind of method forming silica-based product/composition, described method comprises: a. provides silica containing presoma (SCP), and described presoma is included in pH value and is less than or equal in the solution of 7; B. to adulterate described SCP with one or more metallicses alternatively, wherein said being entrained in when solution has the pH value being less than or equal to 7 occurs; C. regulate the pH value of described solution to being greater than 7; D. in described solution, add the salt of significant quantity, so that the electric conductivity of solution is more than or equal to 4mS, wherein said to be added in step 1c pH value regulate before, simultaneously or occur afterwards; E. filter alternatively and dry described SCP; To make in step e dry product and functional group reactions alternatively with f., and the desciccate that wherein gained is functionalized is alternatively at least one in following material: functionalized metal oxide-doping or the silica product of metallic sulfide-doping.
Present invention also offers a kind of method forming silica-based product/composition, described method comprises: a. provides silica containing presoma (SCP), and described presoma is included in pH value and is greater than in the solution of 7; B. regulate the pH value of described solution to being less than or equal to 7; C. to adulterate described SCP with one or more metallicses alternatively, wherein said being entrained in when described solution has the pH value being less than or equal to 7 occurs; D. regulate the pH value of described solution to being greater than 7; E. add the salt of significant quantity to described solution, so that the electric conductivity of described solution is more than or equal to 4mS, wherein said to be added in step 2d pH value regulate before, simultaneously or occur afterwards; F. filter alternatively and dry described SCP; To make in step f dry product and functional group reactions alternatively with g., and the desciccate that wherein gained is functionalized is alternatively at least one in following material: functionalized metal oxide-doping or the silica product of metallic sulfide-doping.
Embodiment
Any patent mentioned in the application and the application of announcement are incorporated to herein by reference.
As mentioned above, the invention provides and a kind ofly comprise the composition with sulphur component cpd, be specially and there is following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide.
Compound can be various forms and be various ratio relative to the composition of composition.In addition, various product can comprise the compound that the present invention includes.Such as, the embodiment of following compound can be independent form, can by chemistry and/or the further modification of physical method, or can be incorporated in other products, the such as consumer's goods or Industrial products.
In one embodiment, in water-based slurry, comprise the compound of 3 % by weight to 15 % by weight.
In another embodiment, in the form of wet cake, comprise the compound of 15 % by weight to 40 % by weight.
In another embodiment, in the form of powder, comprise the compound of 40 % by weight to 99 % by weight.
In another embodiment, this compound has the particle diameter of 5 μm to 200 μm, and comprises the nano particle of the 3nm to 500nm of gathering.In another embodiment, this compound has 30m 2/ g to 800m 2the surface-area of/g.
In another embodiment, this compound has the volume of voids of 0.3cc/g to 2.0cc/g.
In another embodiment, the present invention also provides a kind of by filtering the obtained product of water-based material from composition, and said composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; The mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide; And in water-based slurry, wherein comprise this compound of 3 % by weight to 15 % by weight.
In another embodiment, product is by obtained at the temperature drying composition of 100 ° of C to 350 ° of C, and wherein said composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein to exist alternatively and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth; Wherein F exists and described F has at least one in the following material of 0.01% to 100% surface area coverage alternatively: functionalized organosilane, the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide.
Compound can obtain in various manners, and as No. 20070231247th, U.S. Patent Publication, it is incorporated to herein by reference.
As mentioned above, the silica containing product that the present invention includes can be obtained by following methods.
A method comprises from acid starting point.
In one embodiment, the method comprises the silica-based product of formation, and comprise step: a. provides silica containing presoma (SCP), this presoma is included in pH value and is less than or equal in the solution of 7; B. alternatively with one or more metallicses doping SCP, wherein said being entrained in when solution has the pH value being less than or equal to 7 occurs; C. the pH value of regulator solution is to being greater than 7; D. add the salt of significant quantity to solution, so that the electric conductivity of solution is more than or equal to 4mS, wherein said to be added in step 1c pH value regulate before, simultaneously or occur afterwards; E. filter alternatively and dry SCP; To make in step e dry product and functional group reactions alternatively with f., and the desciccate that wherein gained is functionalized is alternatively at least one in following material: functionalized metal oxide-doping or the silica product of metallic sulfide-doping.
In another embodiment, the functional group in step f is organosilane.
In another embodiment, silica containing presoma is selected from least one in following material: the aerosil of silicic acid, silica colloidal, tetraethyl orthosilicate salt and dispersion.
In another embodiment, step 1(a) in the pH value range of SCP be 3 to 4.
In another embodiment, by described SCP molecule and basic solution being mixed with the shearing rate of the 6m/s to 23m/s based on blade end speed/interact and regulating the pH value of SCP to being greater than 7.In another embodiment, the method comprises further by being mixed with basic solution by described SCP with mixing section and regulates the pH value of SCP to being greater than 7.The case history of mixing section in United States Patent (USP) the 7th, in 550, No. 060 " for carrying the method and apparatus (MethodandArrangementforFeedingChemicalsintoaProcessStrea m) of chemical substance in process stream ".This patent is incorporated to herein by reference.In one embodiment, this mixing section comprises first conduit with one or more import and outlet; Have the second conduit of one or more import and outlet, wherein said first conduit is fixed to described second conduit and passes described second conduit; Have the mixing section of one or more import and outlet, wherein said second conduit is fixed to described mixing section and the described outlet of wherein said first conduit is communicated with described mixing section with the described outlet of described second conduit; And be fixed to the interconnecting device of described mixing section with the described outlet of described mixing section.Then this mixing section can be connected with container or be communicated with, and this container holds/process mix products by (such as conduit).In one embodiment, then described mixing section can be connected with container or be communicated with, and this container holds/process the mix products being regulated generation by the described pH value of described SCP.
In addition, can utilize mixing device UltraTurax, model UTI-25(is purchased from Wilmington, NC works, Inc.).
It is contemplated that any suitable reactor or mixing device/room may be used in method of the present invention.
In another embodiment, the method comprises further and causes Reynolds number be more than or equal to 2000 and regulate the pH value of SCP to being greater than 7, to form silica-based product by being combined with basic solution by described SCP to mix simultaneously.
In another embodiment, under the method is included in transition flow condition further, namely Reynolds number is between 2000 to 4000, regulates the pH value of SCP to being greater than 7, to form silica-based product by being combined with basic solution by described SCP.
In another embodiment, under the method is included in turbulent-flow conditions further, namely Reynolds number is more than or equal to 4000, regulates the pH value of SCP to being greater than 7, to form silica-based product by being combined with basic solution by described SCP.
In another embodiment, utilize chemical substance that the pH value of SCP is adjusted to pH value range 7 to 11, described chemical substance is selected from least one in following material: ammonium hydroxide, volatile salt, mineral alkali as but be not limited to sodium hydroxide and/or potassium hydroxide, organic bases as but be not limited to trimethylammonium hydroxide, alkaline silicate, sulphide salt as but be not limited to sodium sulphite and containing polysulfide salt as but be not limited to calcium polysulfide and/or sodium polysulphide.
In another embodiment, the slurry by filtration that obtains in steps d is dry, so that described drying the solids concn of filtration product is increased to about 99wt% from about 5wt%.
In another embodiment, in at least one technique, carry out surface treatment by the hydrolysis and condensation organosilane that control the silane of silica sphere to product dry in step e, described technique is: organic solvent, supercritical solvent or solvent-free process.
Another method comprises from alkaline starting point.
In one embodiment, the method comprises the silica-based product of formation, and comprise step: a. provides silica containing presoma (SCP), this presoma is included in pH value and is greater than in the solution of 7; B. the pH value of regulator solution is to being less than or equal to 7; C. alternatively with one or more metallicses doping SCP, wherein said being entrained in when solution has the pH value being less than or equal to 7 occurs; D. the pH value of regulator solution is to being greater than 7; E. add the salt of significant quantity to solution, so that the electric conductivity of solution is more than or equal to 4mS, wherein said to be added in step 2d pH value regulate before, simultaneously or occur afterwards; F. filter alternatively and dry SCP; To make in step f dry product and functional group reactions alternatively with g., and the desciccate that wherein gained is functionalized is alternatively at least one in following material: functionalized metal oxide-doping or the silica product of metallic sulfide-doping.
In another embodiment, the functional group in step g is organosilane.
In another embodiment, at least one in following material is selected from containing silicon precursor: the aerosil of silicic acid, silica colloidal, alkaline silicate, tetraethyl orthosilicate salt and dispersion.
In another embodiment, by utilizing at least one in following material: carbonic acid, organic acid as but be not limited to acetic acid, mineral acid as but be not limited to sulfuric acid and/or hydrochloric acid, regulate containing the pH value of silicon precursor, so that pH value is down to scope 2 to 7.
In another embodiment, with acetic acid, the pH value range of SCP is adjusted to scope 3 to 4.
In another embodiment, utilize chemical substance that the pH value of SCP is adjusted to pH value range 7 to 11, described chemical substance is selected from least one in following material: ammonium hydroxide, volatile salt, mineral alkali, organic bases, alkaline silicate, sulphide salt and the salt containing polysulfide.
In another embodiment, by also dry for the slurry by filtration obtained in step e, so that the solids concn of described drying and filtration product is increased to about 99wt% by about 5wt%.
In another embodiment, in at least one technique, carry out surface treatment by the hydrolysis and condensation organosilane that control the silane of silica sphere to product dry in step f, described technique is following: organic solvent, supercritical solvent or solvent-free process.
In another embodiment, regulate the pH value of SCP to being greater than 7 by being mixed with the shearing rate of the 6m/s to 23m/s based on blade end speed with basic solution by described SCP molecule.
In another embodiment, the method comprises further by being mixed with basic solution by described SCP with mixing section and regulates the pH value of SCP to being greater than 7.The case history of mixing section in United States Patent (USP) the 7th, in 550, No. 060 " for carrying the method and apparatus (MethodandArrangementforFeedingChemicalsintoaProcessStrea m) of chemical substance in process stream ".This patent is incorporated to herein by reference.In one embodiment, this mixing section comprises first conduit with one or more import and outlet; Have the second conduit of one or more import and outlet, wherein said first conduit is fixed to described second conduit and passes described second conduit; Have the mixing section of one or more import and outlet, wherein said second conduit is fixed to described mixing section and the described outlet of wherein said first conduit is communicated with described mixing section with the described outlet of described second conduit; And be fixed to the interconnecting device of described mixing section with the described outlet of described mixing section.Then this mixing section can be connected with container or be communicated with, and this container holds/process mix products by (such as conduit).In one embodiment, then described mixing section can be connected with container or be communicated with, and this container holds/process the mix products being regulated generation by the described pH value of described SCP.
In addition, can utilize mixing device UltraTurax, model UTI-25(is purchased from Wilmington, NC works, Inc.).
It is contemplated that any suitable reactor or mixing device/room may be used in method of the present invention.
In another embodiment, the method comprises further and causes Reynolds number be more than or equal to 2000 and regulate the pH value of SCP to being greater than 7, to form silica-based product by being combined with basic solution by described SCP to mix simultaneously.
In another embodiment, under the method is included in transition flow condition further, namely Reynolds number is between 2000 to 4000, regulates the pH value of SCP to being greater than 7, to form silica-based product by being combined with basic solution by described SCP.In another embodiment, under the method is included in turbulent-flow conditions further, namely Reynolds number is more than or equal to 4000, regulates the pH value of SCP to being greater than 7 to form silica-based product by being combined with basic solution by described SCP.In another embodiment, organosilane is all kinds and usually can by R (4-a)-SiX arepresent, wherein a can be 1 to 3.Organo-functional group R-can be any aliphatic hydrocarbon containing, for example the functional group of propyl group, butyl, 3-chloropropyl and combination thereof or alkene.X represents hydrolyzable alkoxyl group, is generally methoxy or ethoxy.Some examples be 3-thiopropyl with the silane of mercapto propyl group.
In the preparation process of composition of the present invention, add salt and be increased to 4mS to make the electric conductivity of reaction soln.The example of operable salt includes, but are not limited to following at least one: alkali and alkaline halide, vitriol, phosphoric acid salt and nitrate, as S-WAT, Repone K, sodium-chlor, SODIUMNITRATE, calcium sulfate and potassiumphosphate.One skilled in the art will realize that to reach and expect electric conductivity and the significant quantity that adds salt changes according to the salt selected.
Embodiment
Embodiment 1:
In the present embodiment, the silicic acid of the 7wt% of 2180g added containing 450g deionization (DI) water and 150g silicic acid and be heated in the residual solution (heel) of 90 DEG C.Silicic acid delivers to 5L reaction flask by peristaltic pump with 10ml/min 3h.
In the DI water of 24.6g, preparation is containing the 25wt% ammonia solution of 16.4g and the solution of 5.84g volatile salt.When the viscosity of solution obviously increases, this solution is added in reaction flask fast.Stir this mixture 30 minutes, then send into any remaining silicic acid with 20ml/min.When silicic acid has been carried, turn off and heated and solution is cooled.
By the filtration of silicon-dioxide slurry and 300 ° of C freeze-drying with production dry powder.From the nitrogen adsorption analysis Autosorb-lC unit of Quantachrome carrying out powder.This sample degassed 2 hours of 300 ° of C, then by the test of multiple spot BET(Brunauer, Emmett and Teller-surface-area) surface-area, pore volume sum BJH(Barrett-Joyner-Halenda) adsorb aperture distribution table and levy.Physical data is shown as the aperture of the surface-area of 354 square metres every gram, the volume of voids of 1.19cc/g and 13.5nm.
Embodiment 2:
In the present embodiment, prepare three kinds of solution: A) 100g nail (unit of length) section N8691 silicon sol, B) be dissolved in 3g Glacial acetic acid in the DI water of 50g and C) be dissolved in the ammonia of the 25wt% of 2.7g volatile salt in the DI water of 150g and 7.5g.Solution B is added solution A, then adds solution C subsequently with high shear rate.Stir this mixture before filtration 1 to 2 minute.Nail (unit of length) section N8691 can from Ondeo Nalco Co., and 1601WestDiehlRoad, Naperville, IL.60563 obtain.
By the filtration of silicon-dioxide slurry and 300 ° of C dryings with production dry powder.Nitrogen adsorption analysis is being carried out from the Autosorb-lC unit of Quantachrome.This sample, degassed 2 hours of 300 ° of C, then adsorbs aperture distribution table by multiple spot BET surface-area, pore volume sum BJH and levies.Nitrogen adsorption analysis is shown as the aperture of the surface-area of 240 square metres every gram, the volume of voids of 0.57cc/g and 9.6nm.
Embodiment 3:
In the present embodiment, prepare three kinds of solution: A) the nail (unit of length) section N8691 silicon sol of 100g, B) be dissolved in the poly aluminium chloride of 3g Glacial acetic acid in the DI water of 50g and 11.8g and C) be dissolved in the ammonia of the 25wt% of the 15g in the DI water of 150g.Solution B added solution A and mixes, then adding solution C subsequently with high shear rate.Stir this mixture before filtration 1 to 2 minute.
The silicon-dioxide slurry adulterated by Al-filters and 300 ° of C dryings with production dry powder, is then carrying out nitrogen adsorption analysis from the Autosorb-lC unit of Quantachrome.This sample, degassed 2 hours of 300 ° of C, then adsorbs aperture distribution table by multiple spot BET surface-area, pore volume sum BJH and levies.Nitrogen adsorption analysis is shown as the aperture of the surface-area of 469 square metres every gram, the volume of voids of 0.82cc/g and 7.0nm.
the combination of composition described in patent application
In one embodiment, the composition of claim to a product comprises adsorbent elements and compositions related various combinations, as formed the mol ratio of particle.In further embodiment, claimed composition comprises the combination of dependent claims.In further embodiment, the scope of concrete composition or its equivalent scope should comprise the separate constituent within the scope of this or the scope within the scope of this.
In another embodiment, the claim of using method comprises adsorbent elements and compositions related various combinations, as formed the mol ratio of particle.In further embodiment, claimed using method comprises the combination of dependent claims.In further embodiment, the scope of concrete composition or its equivalent scope should comprise the separate constituent within the scope of this or the scope within the scope of this.
In another embodiment, the claim of manufacture method comprises adsorbent elements and compositions related various combinations, as pH controls.In further embodiment, claimed using method comprises the combination of dependent claims.In further embodiment, the scope of concrete composition or its equivalent scope should comprise the separate constituent within the scope of this or the scope within the scope of this.

Claims (10)

1. a composition, described composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein, M exists alternatively and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth; Wherein F exists and described F is the functionalized organosilane with 0.01% to 100% surface area coverage alternatively; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide; And wherein said compound has the particle diameter of 5 μm to 200 μm,
Wherein, described functionalized organosilane is at least one in following material: the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl.
2. composition as claimed in claim 1, wherein comprises the compound of 3 % by weight to 15 % by weight in water-based slurry.
3. composition as claimed in claim 1, wherein comprises the compound of 15 % by weight to 40 % by weight in the form of wet cake.
4. composition as claimed in claim 1, wherein comprises the compound of 40 % by weight to 99 % by weight in the form of powder.
5. composition as claimed in claim 4, wherein said compound comprises the nano particle of the 3nm to 500nm of gathering.
6. composition as claimed in claim 4, wherein said compound has 30m 2/ g to 800m 2the surface-area of/g.
7. composition as claimed in claim 4, wherein said compound has the volume of voids of 0.3cc/g to 2.0cc/g.
8., by filtering the obtained product of water-based material from composition, described composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F is the functionalized organosilane with 0.01% to 100% surface area coverage alternatively; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide; And in water-based slurry, wherein comprise the described composition of 3 % by weight to 15 % by weight; And wherein said compound has the particle diameter of 5 μm to 200 μm,
Wherein, described functionalized organosilane is at least one in following material: the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl.
9., by the product that the temperature drying composition at 100 DEG C to 350 DEG C is obtained, wherein said composition comprises and has following general formula (SiO 2) x(OH) ym zo athe compound of F: wherein M exists and described M is at least one in following metal or metalloid positively charged ion: boron, magnesium, aluminium, calcium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, molybdenum, palladium, silver, cadmium, tin, platinum, gold and bismuth alternatively; Wherein F exists and described F is the functionalized organosilane with 0.01% to 100% surface area coverage alternatively; And the mol ratio that wherein mol ratio of y/x equals 0.01 to 0.5, x/z equals 0.1 to 300, and the mol ratio of a/z depends on the character of formed metal oxide; And wherein said compound has the particle diameter of 5 μm to 200 μm,
Wherein, described functionalized organosilane is at least one in following material: the organosilane of sulfur-bearing, the organosilane containing amine and the organosilane containing alkyl.
10. composition as claimed in claim 1, the mol ratio of wherein said x/z be following at least one: 0.56,3.5 and 5.5.
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